تفاعل #595303

معادلة التفاعل

1-(trifluoromethyl)cyclopropanamine

diisopropylethylamine

succinic anhydride

→

4-oxo-4-{[1-(trifluoromethyl)cyclopropyl]amino}butanoic acid

المذيبات

dioxane

ظروف التفاعل

المعالجة

1. 1
   workup.WAITto stand overnight at this temperature
2. 2
   workup.STIRRINGAgain, stirring
3. 3
   workup.WAITwas continued for 20 min at 80° C.
4. 4
   درجة الحرارةto cool to room temperature
5. 5
   تركيزthe solution was concentrated
6. 6
   غسيلRepeatedly, the solution was washed alternately with ethyl acetate and with water
7. 7
   أخرىThe combined organic phases were dried
8. 8
   تركيزconcentrated

الإجراء التجريبي

Slowly, 800.7 mg (4.96 mmol) of 1-(trifluoromethyl)cyclopropanamine and 0.85 ml (4.96 mmol) of diisopropylethylamine were added to a solution of 496 mg (4.96 mmol) of succinic anhydride in 10 ml of dioxane, with ice-cooling (10° C.). Stirring was continued for 20 min at room temperature, and the mixture was allowed to stand overnight at this temperature. Again, stirring was continued for 20 min at 80° C., the mixture was allowed to cool to room temperature, and the solution was concentrated. Repeatedly, the solution was washed alternately with ethyl acetate and with water. The combined organic phases were dried and concentrated. This gave 815.8 mg (73% of theory) of the desired compound.

المصدر